HRID11977

反应详情

EQUATION

反应方程式

HRID 11977 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
35 °C

PROCEDURE

实验过程

265.2 mL (1.95 mol, 525.353 g) bromopentafluorobenzene, 52.11 g (2.144 mol) magnesium powder and 216 mL (0.975 mol, 203.025 g) tetraethoxysilane are mixed together at room temperature and diethylether is added dropwise to the vigorously stirred solution until an exothermic reaction is observed (˜240 ML). The solution is stirred for 30 minutes after which additional 90 mL of Et2O is carefully added. After stirring at 35° C. for 16 h the mixture is cooled to room temperature and diethylether evaporated. An excess of n-heptane (˜600 mL) is added to precipitate the magnesium salts. Solution is filtrated and evaporated to dryness. The residue is fractionally distilled under reduced pressure to yield di(pentafluorophenyl)diethoxysilane.

WORKUP

后处理

  1. additionis carefully added
  2. temperatureis cooled to room temperature
  3. customdiethylether evaporated
  4. additionAn excess of n-heptane (˜600 mL) is added
  5. customto precipitate the magnesium salts
  6. filtrationSolution is filtrated
  7. customevaporated to dryness
  8. distillationThe residue is fractionally distilled under reduced pressure